Method of making unfreezable explosives.



"units VEZIO vnnnza n, or rattan; trans.

METHOD OI IIIAKING UNFREEZA'BLE EXZLOSIVES.

filed October 30, 1909.,

To (ZZZ whom it may} concern:

Be it known that I, Vnzro Yunnan, a'subject of the King of Italy, residing at Milan, Italy, have invented certain new and useful Improvements in Methods of Making U11 treezable Explosives, of which the following' is a specification.

The present invention has for its objectprimarily to provide a method of making practically unfreezable explosives having a plastic and horny consistency and a low explosive temperature.

At the present time it is regarded as essential that explosives and smokeless powder have a plastic and horny consistency, but such substances as have been heretofore made containing nitro-glycerin are objectionable in that they freeze at a temperature below 50 1 they lose their valuable'jprop crties and they are also slow of ignition and are very dangerous.

The present invention relates to the preparation and the use of nitrate'd esters of glycerin with formic or acetic acid, nitroknown in that they are not volatile sub-' Y stances but arevery permanent, they do not contain clilorin, they are not hygroscopic and, moreover, are easy to make.

' free OH} 7 3 I nitrating acetins (containing with ordinary 'nitro sulfuric acid for maliing nitro-glycerin, a Very poor' yield of nitroglycerin is obtainedwhich moreover Specification of Letters Fatent,

contains little nitracetin. 'It'has-beenfoundthat the sulfuric acid of the acid mixture separates acetyl, and that on the other hand, a good yield of pure nitracetin can be obtaincdhy nitrating the basic acetins with nitric acid of more than NO 'H or with nitro-sulturic acid containing more nitric than sulfuric acid, and that a good yield of mixtures of nitracetin and intro-glycerin can be obtained by nitrating acetin-glycerin mixtures, if acid mixtures are employed containing as much more nitric acid than sulfuric acid as there is acetin in propor-.

tion to lvccri. 13v obtainin 'iurc nitraceh c: tins, as nuntioncdabove, it has been drscox cred that these nitracetins possess certain valuable properties which areof especial Patented June 313, T932 Serial Ho. 525,545.

' no Drawing. ori inal application filed December a, was, Serial No. 346,961. named and this application 1 I I fll 'utility in the manufactureof explosives,

that to say, it has been found that ni tracetln does not freeze even. at- .very low temperatures nor does nitracetin'freeze at,

very low temperatures when mixedavith nitro-glycerin th atnitra-cetin is extremely nonsusceptible to heat and shock audit is so great a solvent for gun cotton even when cold that gun cotton'of'l3. l%;,N may be gelatinizedg Moreover, dinitra' cetin can not be exploded or ignited by means of a hammer or by striking 'ironaga'inst iron, but when expldcled with a suitable primer, it

possesses airexplosive power as great asnitro-g-lyceriualthough it has a lower ex- 'plosion temperature. Nitro-formins here: tofore unknown can also be obtained by nitrat-ing formin, and it has been found that these nitro-formins have'a great explosive power and they also lower the freezing point of nitroglycerin to such ail-extent that a mixture for-instance of about 25% clinit-ro-tormin with nitro-glycerin may be regarded as practically untreezable.

h Iore specifically, the invention may be disclosed more clearly by the following which are given as examples 4 Example No. 1: 100 kgs. of glycerin 99%) are heated with 20 kgs. of anhydrous oxalic acid at 100 C. and the mixture is the'nlheated for about '20 hours at a temperature'ranging between 1&0 and 150 (1., the product obtained which consists of about 125 kgs. of a mixture of formin and glycerin is directly nitrated in 275' kgs. of nitric acid:

(96%) and 90 kgs. of fuming sulfuric acid (25% S0 at 25? C. after which the oil separated after washing with water and a warm soda-solution'is of a pale yellow color vand has'a specific gravity of 1.57 at- 15 C. and aboutl5.7% N corresponding to a mixture'of initro-formin and 672 trinitroglycerin. ,100 kgs. of this intro-glycerin mixture is gelatinized with 10 kgs. of colic clion cotton to obtain-a blasting gelatin or with 200 lags. of nitro-cellulose to obtain horny explosives, the blasting gelatin. or

horny explosives thus obtained. remaining.

unfrozen even at a temperature of minus 17 C.

llixample No. 2: 100K kgs. orglycerin (9992) and Takes. acetic acid (99%;).336 boiled for about 2% hours and acetic acid is distilled off by heating to 240 0.; t" the raw monacetin obtained, l25.;hg-s:

are in tinted with 340 kgs. of nitric acid of and 110 kgs. fuming sulfuric acid (25%;:- SO at 25 C.; the whole'is poured into Water'and the separatedoil Washed with Water and a Warm soda solution. A pale yellow oil having a specific gravity of 1.45 at 15 C. is obtained which is insoluble in water; benzin and sulfid of carbon,' s0luble' r r .1n nitric acid, alcohol, acetone and n1tr0-' T /anzyl test an. expansion of about 450 glycerin, consisting in nitrating a suitable flbasicglycerin ester of a nonobesic acid of the acetic series with acidcontainlng not less tain iirzibtically. unfreczable explosives.

*2. A method of making mixed esters of glycerin, consisting in nitmting a suitable basic glycerin ester of 'a 'monobasic acid of 25 the acetic series With amixture of nitric and sulfuric acid, containing more nitric than Y sulfuric zicidJ In testirnony whereof I have hereunto set my hand in presence of two subscribing Wit 30 nesses.

I VEZIO VENDER.

\Vitnesses:

N. LYLE RoBB, CHAS. H. FLISCHER. 

